CN116161946B - Method for preparing ceramic tile with antifouling effect by taking recycled waste as raw material - Google Patents
Method for preparing ceramic tile with antifouling effect by taking recycled waste as raw material Download PDFInfo
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- CN116161946B CN116161946B CN202211690906.1A CN202211690906A CN116161946B CN 116161946 B CN116161946 B CN 116161946B CN 202211690906 A CN202211690906 A CN 202211690906A CN 116161946 B CN116161946 B CN 116161946B
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- 239000000919 ceramic Substances 0.000 title claims abstract description 50
- 239000002699 waste material Substances 0.000 title claims abstract description 39
- 230000003373 anti-fouling effect Effects 0.000 title claims abstract description 34
- 239000002994 raw material Substances 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 title claims abstract description 24
- 238000011282 treatment Methods 0.000 claims abstract description 97
- 238000003756 stirring Methods 0.000 claims abstract description 73
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 62
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 58
- 229910021393 carbon nanotube Inorganic materials 0.000 claims abstract description 58
- 239000010456 wollastonite Substances 0.000 claims abstract description 55
- 229910052882 wollastonite Inorganic materials 0.000 claims abstract description 55
- 239000003607 modifier Substances 0.000 claims abstract description 28
- 238000002156 mixing Methods 0.000 claims abstract description 26
- 229920001661 Chitosan Polymers 0.000 claims abstract description 24
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 18
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 15
- 238000001132 ultrasonic dispersion Methods 0.000 claims abstract description 13
- 238000000227 grinding Methods 0.000 claims abstract description 9
- ODBLHEXUDAPZAU-UHFFFAOYSA-N isocitric acid Chemical compound OC(=O)C(O)C(C(O)=O)CC(O)=O ODBLHEXUDAPZAU-UHFFFAOYSA-N 0.000 claims abstract description 9
- SOBHUZYZLFQYFK-UHFFFAOYSA-K trisodium;hydroxy-[[phosphonatomethyl(phosphonomethyl)amino]methyl]phosphinate Chemical compound [Na+].[Na+].[Na+].OP(O)(=O)CN(CP(O)([O-])=O)CP([O-])([O-])=O SOBHUZYZLFQYFK-UHFFFAOYSA-K 0.000 claims abstract description 9
- 239000005995 Aluminium silicate Substances 0.000 claims abstract description 8
- 235000012211 aluminium silicate Nutrition 0.000 claims abstract description 8
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 claims abstract description 8
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims abstract description 8
- VQEHIYWBGOJJDM-UHFFFAOYSA-H lanthanum(3+);trisulfate Chemical compound [La+3].[La+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O VQEHIYWBGOJJDM-UHFFFAOYSA-H 0.000 claims abstract description 8
- 238000011418 maintenance treatment Methods 0.000 claims abstract description 8
- 229910052863 mullite Inorganic materials 0.000 claims abstract description 8
- 239000000454 talc Substances 0.000 claims abstract description 8
- 235000012222 talc Nutrition 0.000 claims abstract description 8
- 229910052623 talc Inorganic materials 0.000 claims abstract description 8
- 239000000243 solution Substances 0.000 claims description 35
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 28
- 238000006243 chemical reaction Methods 0.000 claims description 25
- 238000001035 drying Methods 0.000 claims description 24
- 238000005406 washing Methods 0.000 claims description 24
- 229910052739 hydrogen Inorganic materials 0.000 claims description 21
- 239000001257 hydrogen Substances 0.000 claims description 21
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 20
- 239000002243 precursor Substances 0.000 claims description 17
- 238000002360 preparation method Methods 0.000 claims description 17
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 15
- 229920002545 silicone oil Polymers 0.000 claims description 15
- 239000000463 material Substances 0.000 claims description 12
- 239000011259 mixed solution Substances 0.000 claims description 12
- 239000000758 substrate Substances 0.000 claims description 12
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 10
- 239000007853 buffer solution Substances 0.000 claims description 10
- 150000002431 hydrogen Chemical class 0.000 claims description 9
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 8
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 8
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 8
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 7
- 238000005245 sintering Methods 0.000 claims description 7
- 235000010413 sodium alginate Nutrition 0.000 claims description 7
- 239000000661 sodium alginate Substances 0.000 claims description 7
- 229940005550 sodium alginate Drugs 0.000 claims description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 230000001678 irradiating effect Effects 0.000 claims description 6
- 230000035484 reaction time Effects 0.000 claims description 6
- 238000007873 sieving Methods 0.000 claims description 6
- 230000036632 reaction speed Effects 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims 2
- 230000006872 improvement Effects 0.000 abstract description 7
- 230000002195 synergetic effect Effects 0.000 abstract description 5
- 238000010306 acid treatment Methods 0.000 abstract description 2
- 239000003795 chemical substances by application Substances 0.000 abstract description 2
- 230000035699 permeability Effects 0.000 abstract description 2
- 230000003213 activating effect Effects 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 10
- 230000000694 effects Effects 0.000 description 6
- 239000008055 phosphate buffer solution Substances 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000003068 static effect Effects 0.000 description 2
- 239000006004 Quartz sand Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000003870 refractory metal Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B33/00—Clay-wares
- C04B33/02—Preparing or treating the raw materials individually or as batches
- C04B33/13—Compounding ingredients
- C04B33/132—Waste materials; Refuse; Residues
- C04B33/1324—Recycled material, e.g. tile dust, stone waste, spent refractory material
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B33/00—Clay-wares
- C04B33/02—Preparing or treating the raw materials individually or as batches
- C04B33/04—Clay; Kaolin
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B33/00—Clay-wares
- C04B33/02—Preparing or treating the raw materials individually or as batches
- C04B33/13—Compounding ingredients
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B33/00—Clay-wares
- C04B33/02—Preparing or treating the raw materials individually or as batches
- C04B33/13—Compounding ingredients
- C04B33/1305—Organic additives
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- C04B33/00—Clay-wares
- C04B33/02—Preparing or treating the raw materials individually or as batches
- C04B33/13—Compounding ingredients
- C04B33/131—Inorganic additives
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3427—Silicates other than clay, e.g. water glass
- C04B2235/3436—Alkaline earth metal silicates, e.g. barium silicate
- C04B2235/3454—Calcium silicates, e.g. wollastonite
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/52—Constituents or additives characterised by their shapes
- C04B2235/5284—Hollow fibers, e.g. nanotubes
- C04B2235/5288—Carbon nanotubes
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6562—Heating rate
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6567—Treatment time
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- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/60—Production of ceramic materials or ceramic elements, e.g. substitution of clay or shale by alternative raw materials, e.g. ashes
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Dispersion Chemistry (AREA)
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- Organic Chemistry (AREA)
- Environmental & Geological Engineering (AREA)
- Inorganic Chemistry (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The invention relates to the technical field of ceramic tiles, and in particular discloses a method for preparing a ceramic tile with an antifouling effect by taking recycled waste as a raw material, which comprises the following steps: taking 45-55 parts of tile waste, carrying out pre-improvement treatment, then adding 10-20 parts of mullite, 3-6 parts of calcined talcum and 2-4 parts of kaolin, and stirring and mixing uniformly. According to the invention, the ceramic tile is prepared from the ceramic tile recovered waste material serving as a raw material through grinding treatment and hydrochloric acid solution treatment, and wollastonite with a needle-shaped structure is arranged in a synergistic manner through carbon nano tubes through activating treatment, so that the antifouling performance of the prepared ceramic tile is remarkably improved; the ceramic tile is optimized and improved by the treatment modifier, the treatment modifier is matched with chitosan, trisodium isocitrate, lanthanum sulfate and the like, the nitric acid treatment is carried out, the permeability of the treatment agent is high, the better assembly of ceramic tile raw materials is promoted, and the antifouling performance of the ceramic tile is further enhanced after ultrasonic dispersion and high-pressure maintenance treatment.
Description
Technical Field
The invention relates to the technical field of antifouling ceramic tiles, in particular to a method for preparing a ceramic tile with an antifouling effect by taking recycled waste as a raw material.
Background
The ceramic tile is made of refractory metal oxide and semi-metal oxide, and through grinding, mixing, pressing, glazing and sintering, and is one kind of ceramic, stone, etc. with acid and alkali resistance. The raw materials are mostly mixed by clay and quartz sand after high temperature compression, and the like, and the high-hardness ceramic material has high hardness.
The tile waste has excellent utilization value, but the existing tile waste is low in treatment efficiency after recycling, the utilization technology is poor, and the tile product is low in antifouling performance, so that the tile product cannot be well utilized, and the tile waste is further improved.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a method for preparing a ceramic tile with an antifouling effect by taking recycled waste as a raw material, so as to solve the problems in the prior art.
The invention solves the technical problems by adopting the following technical scheme:
the invention provides a method for preparing a ceramic tile with an antifouling effect by taking recycled waste as a raw material, which comprises the following steps:
step one: taking 45-55 parts of tile waste, pre-improving, adding 10-20 parts of mullite, 3-6 parts of calcined talcum and 2-4 parts of kaolin, and stirring and mixing uniformly;
step two: adding 3-6 parts of carbon nano tube modified wollastonite, and continuously stirring and fully mixing to obtain a material to be used;
step three: then the materials to be used are sent into a grinder to be ball-milled and sieved by a 100-mesh sieve, and then pressed and formed;
step four: then sintering at 1250-1300 ℃ for 1-3h, finally maintaining the temperature at 1050 ℃ at a speed of 1-3 ℃/min for 20-30min, and finally air-cooling to room temperature to obtain the ceramic tile substrate;
and fifthly, placing the ceramic tile substrate in a treatment modifier, performing ultrasonic dispersion treatment, performing high-pressure maintenance treatment, and finally washing and drying to obtain the ceramic tile with the antifouling effect.
Preferably, the method of the pre-improvement treatment is as follows:
grinding the tile waste in a grinder, sieving with 50-100 meshes, then sending into hydrochloric acid solution with the mass fraction of 6-10% and the weight of 3-6 times, stirring and dispersing uniformly, washing with water, and drying.
Preferably, the preparation method of the carbon nano tube modified wollastonite comprises the following steps:
s01: placing 10-15 parts of wollastonite into 20-30 parts of deionized water, adding 3-5 parts of silane coupling agent KH560 and 1-3 parts of sodium dodecyl benzene sulfonate, uniformly stirring, and finally adding 0.6-0.8 part of methyl high-hydrogen silicone oil, and fully stirring and mixing to obtain wollastonite mixed solution;
s02: irradiating the carbon nanotube precursor for 10-20min with irradiation power of 350-400W, placing in sodium alginate solution with mass fraction of 10-15% of 3 times of the weight of the precursor, stirring and dispersing uniformly, washing with water, and drying to obtain pre-improved carbon nanotube;
s03: the pre-improved carbon nano tube and wollastonite mixed solution is prepared by the following components in percentage by weight: (5-9) reaction stirring treatment, water washing and drying after the reaction is finished, and obtaining the carbon nano tube modified wollastonite.
Preferably, the methyl high hydrogen silicone oil has hydrogen content of 1.3-1.5% and viscosity of 15-20mm at 25deg.C 2 .s -1 。
Preferably, the reaction stirring treatment in the step S03 has a reaction rotating speed of 1000-1500r/min and a reaction time of 30-40min.
Preferably, the stirring temperature of the reaction stirring treatment in the step S03 is 55-65 ℃.
Preferably, the preparation method of the treatment modifier comprises the following steps:
s101: adding 5-10 parts of chitosan into 10-15 parts of water, then adding 1-3 parts of trisodium isocitrate and 2-4 parts of lanthanum sulfate, stirring and mixing uniformly, and finally adding 0.5-0.9 part of phosphoric acid buffer solution to obtain chitosan treatment solution;
s102: adding 5-10% nitric acid solution into chitosan treatment liquid, and stirring at 500-1000r/min for 20-30min to obtain treatment modifier.
The inventor of the invention finds that the pollution-resistant level of the product is poor without adding the carbon nano tube modified wollastonite, meanwhile, the static friction coefficient is obviously reduced, the carbon nano tube modified wollastonite is replaced by wollastonite, the performance of the product is poor, in addition, the preparation methods of the carbon nano tube modified wollastonite are different, the performances of the product are different, and the anti-skid and anti-pollution effects on the product are obvious only by adopting the carbon nano tube modified wollastonite prepared by the method of the invention; the inventor of the invention discovers that the treatment of the treatment modifier can synergistically combine the raw materials of the product, and synergistically enhance the antifouling and anti-skid effects of the product; the raw materials are combined, and the synergistic effect of the product is optimal.
Preferably, the pH value of the phosphate buffer solution is 4.5-5.5; the mass fraction of the nitric acid solution is 5-10%.
Preferably, the power of the ultrasonic dispersion treatment in the step five is 350-400W, and the ultrasonic time is 30-40min.
Preferably, the curing pressure of the high-pressure curing treatment in the fifth step is 5-10MPa, the curing temperature is 45-55 ℃, and the curing time is 1-2h.
Compared with the prior art, the invention has the following beneficial effects:
the tile is prepared from tile recovery waste as a raw material by grinding, hydrochloric acid solution treatment, activation treatment and improvement by matching with raw materials such as mullite, calcined talcum, kaolin and the like; the product is optimized by adding the carbon nano tube modified wollastonite, the wollastonite has a needle-shaped structure, the silane coupling agent KH560, sodium dodecyl benzene sulfonate and methyl high hydrogen silicone oil are matched and modified, the silane coupling agent KH560 has an interface modification effect, the sodium dodecyl benzene sulfonate has an active efficiency, the methyl high hydrogen silicone oil is used for anti-fouling modification, the carbon nano tube is subjected to proton irradiation, the activity can be improved, the dispersion degree is improved by dispersing the sodium alginate solution, and the wollastonite with the needle-shaped structure is arranged in a synergistic way through the carbon nano tube after the wollastonite is optimized and modified, so that the anti-fouling performance of the prepared ceramic tile is obviously improved; the ceramic tile is optimized and improved by the treatment modifier, the treatment modifier is matched with chitosan, trisodium isocitrate, lanthanum sulfate and the like, the nitric acid treatment is carried out, the permeability of the treatment agent is high, the better assembly of ceramic tile raw materials is promoted, and the antifouling performance of the ceramic tile is further enhanced after ultrasonic dispersion and high-pressure maintenance treatment.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and fully with reference to the accompanying drawings, in which it is evident that the embodiments described are only some, but not all embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The method for preparing the ceramic tile with the antifouling effect by taking the recycled waste as the raw material comprises the following steps:
step one: taking 45-55 parts of tile waste, pre-improving, adding 10-20 parts of mullite, 3-6 parts of calcined talcum and 2-4 parts of kaolin, and stirring and mixing uniformly;
step two: adding 3-6 parts of carbon nano tube modified wollastonite, and continuously stirring and fully mixing to obtain a material to be used;
step three: then the materials to be used are sent into a grinder to be ball-milled and sieved by a 100-mesh sieve, and then pressed and formed;
step four: then sintering at 1250-1300 ℃ for 1-3h, finally maintaining the temperature at 1050 ℃ at a speed of 1-3 ℃/min for 20-30min, and finally air-cooling to room temperature to obtain the ceramic tile substrate;
and fifthly, placing the ceramic tile substrate in a treatment modifier, performing ultrasonic dispersion treatment, performing high-pressure maintenance treatment, and finally washing and drying to obtain the ceramic tile with the antifouling effect.
The method for pre-improvement treatment of the embodiment comprises the following steps:
grinding the tile waste in a grinder, sieving with 50-100 meshes, then sending into hydrochloric acid solution with the mass fraction of 6-10% and the weight of 3-6 times, stirring and dispersing uniformly, washing with water, and drying.
The preparation method of the carbon nano tube modified wollastonite in the embodiment comprises the following steps:
s01: placing 10-15 parts of wollastonite into 20-30 parts of deionized water, adding 3-5 parts of silane coupling agent KH560 and 1-3 parts of sodium dodecyl benzene sulfonate, uniformly stirring, and finally adding 0.6-0.8 part of methyl high-hydrogen silicone oil, and fully stirring and mixing to obtain wollastonite mixed solution;
s02: irradiating the carbon nanotube precursor for 10-20min with irradiation power of 350-400W, placing in sodium alginate solution with mass fraction of 10-15% of 3 times of the weight of the precursor, stirring and dispersing uniformly, washing with water, and drying to obtain pre-improved carbon nanotube;
s03: the pre-improved carbon nano tube and wollastonite mixed solution is prepared by the following components in percentage by weight: (5-9) reaction stirring treatment, water washing and drying after the reaction is finished, and obtaining the carbon nano tube modified wollastonite.
The methyl high hydrogen silicone oil of this example has a hydrogen content of 1.3-1.5% and a viscosity of 15-20mm at 25deg.C 2 .s- 1 。
The reaction stirring treatment in S03 of the embodiment has a reaction speed of 1000-1500r/min and a reaction time of 30-40min.
The stirring temperature of the reaction stirring treatment in S03 of this example was 55 to 65 ℃.
The preparation method of the treatment modifier of the embodiment comprises the following steps:
s101: adding 5-10 parts of chitosan into 10-15 parts of water, then adding 1-3 parts of trisodium isocitrate and 2-4 parts of lanthanum sulfate, stirring and mixing uniformly, and finally adding 0.5-0.9 part of phosphoric acid buffer solution to obtain chitosan treatment solution;
s102: adding 5-10% nitric acid solution into chitosan treatment liquid, and stirring at 500-1000r/min for 20-30min to obtain treatment modifier.
The pH value of the phosphoric acid buffer solution of the embodiment is 4.5-5.5; the mass fraction of the nitric acid solution is 5-10%.
The power of the ultrasonic dispersion treatment in the step five of the embodiment is 350-400W, and the ultrasonic time is 30-40min.
In the fifth step of the embodiment, the curing pressure of the high-pressure curing treatment is 5-10MPa, the curing temperature is 45-55 ℃ and the curing time is 1-2h.
Example 1.
The method for preparing the ceramic tile with the antifouling effect by taking the recycled waste as the raw material comprises the following steps:
step one: taking 45 parts of tile waste, pre-improving, adding 10 parts of mullite, 3 parts of calcined talcum and 2 parts of kaolin, and uniformly stirring and mixing;
step two: adding 3 parts of carbon nano tube modified wollastonite, and continuously stirring and fully mixing to obtain a material to be used;
step three: then the materials to be used are sent into a grinder to be ball-milled and sieved by a 100-mesh sieve, and then pressed and formed;
step four: then sintering at 1250 ℃ for 1h, finally maintaining the temperature at 1050 ℃ at a speed of 1 ℃/min for 20min, and finally air-cooling to room temperature to obtain the ceramic tile substrate;
and fifthly, placing the ceramic tile substrate in a treatment modifier, performing ultrasonic dispersion treatment, performing high-pressure maintenance treatment, and finally washing and drying to obtain the ceramic tile with the antifouling effect.
The method for pre-improvement treatment of the embodiment comprises the following steps:
grinding tile waste in a grinder, sieving with 50 meshes, then sending into hydrochloric acid solution with the mass fraction of 6-10% which is 3 times of that of the tile waste, stirring and dispersing uniformly, washing with water, and drying.
The preparation method of the carbon nano tube modified wollastonite in the embodiment comprises the following steps:
s01: placing 10 parts of wollastonite into 20 parts of deionized water, adding 3 parts of silane coupling agent KH560 and 1 part of sodium dodecyl benzene sulfonate, uniformly stirring, and finally adding 0.6 part of methyl high-hydrogen silicone oil, and fully stirring and mixing to obtain wollastonite mixed solution;
s02: irradiating the carbon nanotube precursor for 10min, wherein the irradiation power is 350W, and after the irradiation is finished, placing the carbon nanotube precursor into sodium alginate solution with the mass fraction of 10% which is 3 times that of the carbon nanotube precursor, stirring and dispersing uniformly, and finally washing and drying the carbon nanotube precursor to obtain the pre-improved carbon nanotube;
s03: the pre-improved carbon nano tube and wollastonite mixed solution is prepared by the following components in percentage by weight: and 5, carrying out reaction stirring treatment, finishing the reaction, washing with water and drying to obtain the carbon nano tube modified wollastonite.
The methyl highly hydrogen silicone oil of this example had a hydrogen content of 1.3% and a viscosity of 15mm at 25 ℃ 2 .s -1 。
The reaction stirring treatment in S03 of this example was carried out at a reaction speed of 1000r/min and a reaction time of 30min.
The stirring temperature of the reaction stirring treatment in S03 of this example was 55 ℃.
The preparation method of the treatment modifier of the embodiment comprises the following steps:
s101: adding 5 parts of chitosan into 10 parts of water, then adding 1 part of trisodium isocitrate and 2 parts of lanthanum sulfate, stirring and uniformly mixing, and finally adding 0.5 part of phosphoric acid buffer solution to obtain chitosan treatment solution;
s102: adding 5% nitric acid solution into the chitosan treatment liquid, and stirring at 500r/min for 20min to obtain the treatment modifier.
The pH of the phosphate buffer solution of this example was 4.5; the mass fraction of the nitric acid solution is 5%.
In the fifth step of the present embodiment, the power of the ultrasonic dispersion treatment is 350W, and the ultrasonic time is 30min.
In the fifth step of this embodiment, the curing pressure of the high-pressure curing treatment is 5MPa, the curing temperature is 45 ℃, and the curing time is 1h.
Example 2.
The method for preparing the ceramic tile with the antifouling effect by taking the recycled waste as the raw material comprises the following steps:
step one: taking 55 parts of tile waste, pre-improving, adding 20 parts of mullite, 6 parts of calcined talcum and 4 parts of kaolin, and uniformly stirring and mixing;
step two: adding 6 parts of carbon nano tube modified wollastonite, and continuously stirring and fully mixing to obtain a material to be used;
step three: then the materials to be used are sent into a grinder to be ball-milled and sieved by a 100-mesh sieve, and then pressed and formed;
step four: then sintering at 1300 ℃ for 3 hours, finally maintaining the temperature at 1050 ℃ at a speed of 3 ℃/min for 30min, and finally air-cooling to room temperature to obtain the ceramic tile substrate;
and fifthly, placing the ceramic tile substrate in a treatment modifier, performing ultrasonic dispersion treatment, performing high-pressure maintenance treatment, and finally washing and drying to obtain the ceramic tile with the antifouling effect.
The method for pre-improvement treatment of the embodiment comprises the following steps:
grinding the tile waste in a grinder, sieving with 100 meshes, then sending into hydrochloric acid solution with the mass fraction of 10% which is 6 times of the weight of the tile waste, stirring and dispersing uniformly, washing with water, and drying.
The preparation method of the carbon nano tube modified wollastonite in the embodiment comprises the following steps:
s01: 15 parts of wollastonite is placed in 30 parts of deionized water, then 5 parts of silane coupling agent KH560 and 3 parts of sodium dodecyl benzene sulfonate are added, the mixture is stirred uniformly, and finally 0.8 part of methyl high-hydrogen silicone oil is added, and the mixture is stirred fully to obtain wollastonite mixed solution;
s02: irradiating the carbon nanotube precursor for 20min, wherein the irradiation power is 400W, and after the irradiation is finished, placing the carbon nanotube precursor into sodium alginate solution with the mass fraction of 15% which is 3 times that of the carbon nanotube precursor, stirring and dispersing uniformly, and finally washing and drying the carbon nanotube precursor to obtain the pre-improved carbon nanotube;
s03: the pre-improved carbon nano tube and wollastonite mixed solution is prepared by the following components in percentage by weight: and 9, carrying out reaction stirring treatment, finishing the reaction, washing with water and drying to obtain the carbon nano tube modified wollastonite.
The methyl highly hydrogen silicone oil of this example had a hydrogen content of 1.5% and a viscosity of 20mm at 25 ℃ 2 .s -1 。
The reaction stirring treatment in S03 of this example was carried out at a reaction speed of 1500r/min and a reaction time of 40min.
The stirring temperature of the reaction stirring treatment in S03 of this example was 65 ℃.
The preparation method of the treatment modifier of the embodiment comprises the following steps:
s101: adding 10 parts of chitosan into 15 parts of water, then adding 3 parts of trisodium isocitrate and 4 parts of lanthanum sulfate, stirring and uniformly mixing, and finally adding 0.9 part of phosphoric acid buffer solution to obtain chitosan treatment solution;
s102: adding 10% nitric acid solution into the chitosan treatment liquid, and stirring at 1000r/min for 30min to obtain the treatment modifier.
The pH of the phosphate buffer solution of this example was 5.5; the mass fraction of the nitric acid solution is 10%.
In the fifth step of the present embodiment, the power of the ultrasonic dispersion treatment is 400W, and the ultrasonic time is 40min.
In the fifth step of this embodiment, the curing pressure of the high-pressure curing treatment is 10MPa, the curing temperature is 55 ℃, and the curing time is 2 hours.
Example 3.
The method for preparing the ceramic tile with the antifouling effect by taking the recycled waste as the raw material comprises the following steps:
step one: taking 50 parts of tile waste, pre-improving, adding 15 parts of mullite, 4.5 parts of calcined talcum and 3 parts of kaolin, and uniformly stirring and mixing;
step two: adding 4.5 parts of carbon nano tube modified wollastonite, and continuously stirring and fully mixing to obtain a material to be used;
step three: then the materials to be used are sent into a grinder to be ball-milled and sieved by a 100-mesh sieve, and then pressed and formed;
step four: then sintering at 1270 ℃ for 2 hours, finally maintaining the temperature at 1050 ℃ at a speed of 2 ℃/min for 25min, and finally air-cooling to room temperature to obtain a ceramic tile substrate;
and fifthly, placing the ceramic tile substrate in a treatment modifier, performing ultrasonic dispersion treatment, performing high-pressure maintenance treatment, and finally washing and drying to obtain the ceramic tile with the antifouling effect.
The method for pre-improvement treatment of the embodiment comprises the following steps:
grinding the tile waste in a grinder, sieving with 75 meshes, then sending into hydrochloric acid solution with the mass fraction of 8% which is 4.5 times of the weight of the tile waste, stirring and dispersing uniformly, washing with water, and drying.
The preparation method of the carbon nano tube modified wollastonite in the embodiment comprises the following steps:
s01: placing 12.5 parts of wollastonite into 25 parts of deionized water, then adding 4 parts of silane coupling agent KH560 and 2 parts of sodium dodecyl benzene sulfonate, uniformly stirring, and finally adding 0.7 part of methyl high-hydrogen silicone oil, and fully stirring and mixing to obtain wollastonite mixed solution;
s02: irradiating the carbon nanotube precursor for 15min, wherein the irradiation power is 375W, placing the carbon nanotube precursor in sodium alginate solution with the mass fraction of 12.5% which is 3 times of that of the carbon nanotube precursor, stirring and dispersing uniformly, and finally washing and drying to obtain the pre-improved carbon nanotube;
s03: the pre-improved carbon nano tube and wollastonite mixed solution is prepared by the following components in percentage by weight: and 7, carrying out reaction stirring treatment, finishing the reaction, washing with water and drying to obtain the carbon nano tube modified wollastonite.
This embodimentThe hydrogen content of the methyl high hydrogen silicone oil is 1.4 percent, and the viscosity at 25 ℃ is 17.5mm 2 .s -1 。
The reaction stirring treatment in S03 of this example was carried out at a reaction speed of 1250r/min and a reaction time of 35min.
The stirring temperature of the reaction stirring treatment in S03 of this example was 60 ℃.
The preparation method of the treatment modifier of the embodiment comprises the following steps:
s101: adding 7.5 parts of chitosan into 12.5 parts of water, then adding 2 parts of trisodium isocitrate and 3 parts of lanthanum sulfate, stirring and mixing uniformly, and finally adding 0.7 part of phosphoric acid buffer solution to obtain chitosan treatment solution;
s102: adding nitric acid solution with the total amount of 7.5% into the chitosan treatment liquid, and stirring for 25min at the rotating speed of 750r/min to obtain the treatment modifier.
The pH of the phosphate buffer solution of this example was 5.0; the mass fraction of the nitric acid solution was 7.5%.
Step five of the present example was performed with a power of 375W and an ultrasonic time of 35min.
In the fifth step of this example, the curing pressure of the high-pressure curing treatment was 7.5MPa, the curing temperature was 50℃and the curing time was 1.5 hours.
Comparative example 1.
The difference from example 3 was that no carbon nanotube-modified wollastonite was added.
Comparative example 2.
The difference from example 3 is that wollastonite is used instead of carbon nanotube-modified wollastonite.
Comparative example 3.
The difference from example 3 is that no pre-modified carbon nanotube treatment was used in the preparation of the carbon nanotube modified wollastonite.
Comparative example 4.
The difference from example 3 is that no methyl high hydrogen silicone oil is added in the preparation of the carbon nano tube modified wollastonite.
Comparative example 5.
The difference from example 3 is that the pre-modified carbon nanotubes are replaced with carbon nanotubes.
Comparative example 6.
The difference from example 3 is that no treatment with the treatment modifier was used.
Comparative example 7.
The difference from example 3 is that no chitosan is added to the treatment modifier.
Comparative example 8.
The difference from example 3 is the preparation of the treatment modifier:
s101: adding 7.5 parts of chitosan into 12.5 parts of water, then adding 2 parts of trisodium isocitrate, stirring and mixing uniformly, and finally adding 0.7 part of phosphoric acid buffer solution to obtain chitosan treatment solution;
s102: adding hydrochloric acid solution with the total amount of 7.5% into the chitosan treatment liquid, and stirring at the rotating speed of 750r/min for 25min to obtain a treatment modifier; the pH value of the phosphoric acid buffer solution is 5.0; the mass fraction of the nitric acid solution was 7.5%.
Step five of the present example was performed with a power of 375W and an ultrasonic time of 35min.
In the fifth step of this example, the curing pressure of the high-pressure curing treatment was 7.5MPa, the curing temperature was 50℃and the curing time was 1.5 hours.
Detecting antifouling property according to GB/T3810.14-2006 detection;
the products of examples 1-3 and comparative examples 1-8 were subjected to performance testing;
as can be seen from comparative examples 1-8 and examples 1-3; according to the invention, the pollution-resistant level of the product is poor, the static friction coefficient is obviously reduced, the carbon nano tube modified wollastonite is replaced by wollastonite, the performance of the product is poor, in addition, the preparation methods of the carbon nano tube modified wollastonite are different, the performances of the product are different, and the carbon nano tube modified wollastonite prepared by the method has obvious anti-skid and anti-pollution effects on the product; in addition, the treatment of the treatment modifier can synergistically combine the raw materials of the product, and the synergistic effect can jointly enhance the antifouling and anti-skid effects of the product; the raw materials are combined, and the synergistic effect of the product is optimal.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present disclosure describes embodiments, not every embodiment is provided with a separate embodiment, and that this description is provided for clarity only, and that the disclosure is not limited to the embodiments described in detail below, and that the embodiments described in the examples may be combined as appropriate to form other embodiments that will be apparent to those skilled in the art.
Claims (8)
1. A method for preparing a ceramic tile with an antifouling effect by taking recycled waste as a raw material, which is characterized by comprising the following steps:
step one: taking 45-55 parts of tile waste, pre-improving, adding 10-20 parts of mullite, 3-6 parts of calcined talcum and 2-4 parts of kaolin, and stirring and mixing uniformly;
step two: adding 3-6 parts of carbon nano tube modified wollastonite, and continuously stirring and fully mixing to obtain a material to be used;
step three: then the materials to be used are sent into a grinder to be ball-milled and sieved by a 100-mesh sieve, and then pressed and formed;
step four: then sintering at 1250-1300 ℃ for 1-3h, finally reducing to 1050 ℃ at a speed of 1-3 ℃/min, preserving heat for 20-30min, and finally air-cooling to room temperature to obtain the ceramic tile substrate;
step five, placing the ceramic tile substrate in a treatment modifier, performing ultrasonic dispersion treatment, performing high-pressure maintenance treatment, and finally washing and drying to obtain the ceramic tile with the antifouling effect; the preparation method of the carbon nano tube modified wollastonite comprises the following steps:
s01: placing 10-15 parts of wollastonite into 20-30 parts of deionized water, adding 3-5 parts of silane coupling agent KH560 and 1-3 parts of sodium dodecyl benzene sulfonate, uniformly stirring, and finally adding 0.6-0.8 part of methyl high-hydrogen silicone oil, and fully stirring and mixing to obtain wollastonite mixed solution;
s02: irradiating the carbon nanotube precursor for 10-20min with irradiation power of 350-400W, placing in sodium alginate solution with mass fraction of 10-15% of 3 times of the weight of the precursor, stirring and dispersing uniformly, washing with water, and drying to obtain pre-improved carbon nanotube;
s03: the pre-improved carbon nano tube and wollastonite mixed solution is prepared by the following components in percentage by weight: (5-9) reaction stirring treatment, water washing and drying after the reaction is finished, so as to obtain carbon nano tube modified wollastonite; the preparation method of the treatment modifier comprises the following steps:
s101: adding 5-10 parts of chitosan into 10-15 parts of water, then adding 1-3 parts of trisodium isocitrate and 2-4 parts of lanthanum sulfate, stirring and mixing uniformly, and finally adding 0.5-0.9 part of phosphoric acid buffer solution to obtain chitosan treatment solution;
s102: adding 5-10% nitric acid solution into chitosan treatment liquid, and stirring at 500-1000r/min for 20-30min to obtain treatment modifier.
2. The method for preparing the ceramic tile with the antifouling effect by taking recycled waste as a raw material according to claim 1, wherein the method for pre-improving treatment is as follows:
grinding the tile waste in a grinder, sieving with 50-100 meshes, then sending into hydrochloric acid solution with the mass fraction of 6-10% and the weight of 3-6 times, stirring and dispersing uniformly, washing with water, and drying.
3. The method for producing ceramic tiles with antifouling effect from recycled waste material according to claim 1, wherein the methyl high hydrogen silicone oil has a hydrogen content of 1.3-1.5% and a viscosity of 15-20mm at 25 °c 2 ·s -1 。
4. The method for preparing the ceramic tile with the antifouling effect by using the recycled waste as the raw material according to claim 1, wherein the reaction speed of the reaction stirring treatment in the step S03 is 1000-1500r/min, and the reaction time is 30-40min.
5. The method for producing ceramic tiles having an antifouling effect by using recycled waste as a raw material according to claim 4, wherein the stirring temperature of the reaction stirring treatment in S03 is 55 to 65 ℃.
6. The method for preparing ceramic tiles with antifouling effect by using recycled waste as raw material according to claim 1, wherein the pH value of the phosphoric acid buffer solution is 4.5-5.5; the mass fraction of the nitric acid solution is 5-10%.
7. The method for preparing the ceramic tile with the antifouling effect by taking the recycled waste as the raw material according to claim 1, wherein the power of the ultrasonic dispersion treatment in the step five is 350-400W, and the ultrasonic time is 30-40min.
8. The method for preparing the ceramic tile with the antifouling effect by taking the recycled waste as the raw material according to claim 1, wherein the curing pressure of the high-pressure curing treatment in the fifth step is 5-10MPa, the curing temperature is 45-55 ℃ and the curing time is 1-2h.
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